• Title/Summary/Keyword: A new reagent

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Facile Reduction of Carboxylic Acid Salts to Aldehydes by Boron Hydrides Thexylbromoborane-Dimethyl Sulfide and 9-Borabicyclo [3.3.1]nonane

  • Cha, Jin-Soon;Lee, Kwang-Woo;Yoon, Mal-Sook;Lee, Jae-Cheol;Kim, Jin-Euog
    • Bulletin of the Korean Chemical Society
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    • v.9 no.6
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    • pp.384-388
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    • 1988
  • New methods of the reduction of carboxylic acid salts to aldehydes with 2 equiv of thexylbromoborane-dimethyl sulfide (ThxBHBr${\cdot}SMe_2$) or 9-borabicyclo[3.3.1]nonane (9-BBN) are described. Both these reagents provide the corresponding aldehydes from various as sodium and lithium salts of carboxylic acids in high yields both at room temperature. Such facile reductions are explained as the simple substitution for the bromo group of ThxBHBr by a carboxylate to form thexyl(acyloxty)borane followed by reduction with excess reagent and the formation of an ate complex followed by reduction with excess 9-BBN.

Change of the Result Value by the Amount of Samples in CA 19-9 (CA 19-9 검체량에 따른 농도의 변화)

  • Chang, Hyun-Yeong;Park, Hee-Won;You, Tae-Min;Noh, Kyung-Woon;Kim, Hyun-Joo
    • The Korean Journal of Nuclear Medicine Technology
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    • v.12 no.1
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    • pp.66-73
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    • 2008
  • Purpose: CA 19-9 need to examine a number of sample volume, and the postwar 200 U/ml concentration hook effect appears slight. Thus, the antibody-antigen reaction, and by reducing the amount of (sample volume), they can hook effect to minimize the impact of the sample volume and relevance know, I saw the hook effect. In addition, the current maximum of using the standard concentration of the reagent in 240 U/ml increase more than the standard concentration can be seen knows. Material and Method: 5 U/ml and under, make a few low concentration of serum pool from the high concentration of the sample hook effect together with a standard concentration of about 500 to meet the production. The reagents used in experiments are currently using SNUH NM experiment. Orignal method along with the experiment is to 25 ul sample volume (1 / 4), 50 ul (1 / 2), 100 ul (Orignal method) in the experiment. My greatest concentration of the reagent concentration of approximately two times the standard concentration of production. When was the last to make the first experiment, as measured by the standard concentration after that. The new inspection information through a standard solution modified by entering values in them. Results: 100 ul, and to apply the new standard concentration y = 1.3021x - 10.97, $R^2$ = 0.9844. Overall, the results showed a similar orignal method. Because of the concentration in the value of more than 240 U/ml, but it is an overall value that can be made out of a similar value When I put the 50 ul y = 1.045x + 9.5861, $R^2$ = 0.9428. Overall orignal method and the results of a similar value. 50 ul, and to apply the new standard concentration y=1.2006x+11.252, $R^2$=0.9423. Showing a slightly lower value compared with orignal method. Because of the concentration in the value of more than 240 U/ml, but it is an overall value that can be made out of a similar value. When I put the man 25 ul y=0.6012x+24.755, $R^2$=0.4033. Results showed that very small amounts of sample are insecure inside and showed a lower middle cpm orignal method and showed a lot of mismatched. Conclusions: 25 ul of the sample volume is not possible to use the instability had, when I put the 50 ul of the orignal method can be used to show a similar concentration. The new values are slightly lower concentration, The new values are slightly lower concentration, concentration, which are likely due to the lack of data has had a little gap between the sample showed 80 to 200 U/ml additional experiments seem to do. Apply a new 100 ul concentration values are applied to a large crowd is not even in sight. But this way the concentration of 100 to more 400 U/ml gather further experiments should possible adds.

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Development of a New Approach to Determine the Potency of Bacille Calmette-Guérin Vaccines Using Flow Cytometry

  • Gweon, Eunjeong;Choi, Chanwoong;Kim, Jaeok;Kim, Byungkuk;Kang, Hyunkyung;Park, Taejun;Ban, Sangja;Bae, Minseok;Park, Sangjin;Jeong, Jayoung
    • Osong Public Health and Research Perspectives
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    • v.8 no.6
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    • pp.389-396
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    • 2017
  • Objectives: To circumvent the limitations of the current golden standard method, colony-forming unit (CFU) assay, for viability of Bacille Calmette-$Gu{\acute{e}}rin$ (BCG) vaccines, we developed a new method to rapidly and accurately determine the potency of BCG vaccines. Methods: Based on flow cytometry (FACS) and fluorescein diacetate (FDA) as the most appropriate fluorescent staining reagent, 17 lots of BCG vaccines for percutaneous administration and 5 lots of BCG vaccines for intradermal administration were analyzed in this study. The percentage of viable cells measured by flow cytometry along with the total number of organisms in BCG vaccines, as determined on a cell counter, was used to quantify the number of viable cells. Results: Pearson correlation coefficients of FACS and CFU assays for percutaneous and intradermal BCG vaccines were 0.6962 and 0.7428, respectively, indicating a high correlation. The coefficient of variation value of the FACS assay was less than 7%, which was 11 times lower than that of the CFU assay. Conclusion: This study contributes to the evaluation of new potency test method for FACS-based determination of viable cells in BCG vaccines. Accordingly, quality control of BCG vaccines can be significantly improved.

위령선의 성분연구 제2보 Clematis brachyura Maxim의 flavone에 대하야

  • heo, Geom;Park, Su-Seon
    • YAKHAK HOEJI
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    • v.2 no.1_2
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    • pp.11-15
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    • 1953
  • Two flavons, which are a new flavon (the Authors are going to call it "CLEMATISIN") and a yellow crystalline flavon, are isolated from leaves of Clematis brachura Maxim. Clamatisin : A colorless needle crystal which has a Slightly sweet taste, mp 225 .deg.C (decomp). It is positive (Cherry red) for the Mg-HCl(Hg) reaction and is positive (purple) for the $FeCL_{3}$ reagent. It is soluble easily in methanol, ether, acetone, prydine, ethylacetate, hot water and alkali-solutions. It is soluble slightly in cold water and is insoluble in chloroform, benzene and toluence. According to the results of elementry analysis and molecular weight determination the formula of clematisin agrees with $C_{18}H_{18}O_{7}$ when dried at $80^{\circ}C$, crystalline clematisin (from water) contains one molecule of crystalline water. The following derivatives are prepared ; Clematisin-oxim; a colorless needle crystal, mp 215-216 .deg.C, Clematisin methylate; prepared by diazomethan. mp 191-$192^{\circ}C$ a colorless needle crystal. Acethylmethylate; a colorless powder, It is not sharp in melting point and melts at approximately $215^{\circ}C$, Yellow Crystalline Flavon; mp 285-$286^{\circ}C$ (dexo-mp.), yellow needle crystal. It has a slightly sweet teste and shows positive reaction Acetate; a colorless needle crystal, mp $168^{\circ}C$.

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The Use of Phenanthraquinone Monophenyl Thiosemicarbazone for Preconcentration, Ion Flotation and Spectrometric Determination of Zinc(II) in Human Biofluids and Pharmaceutical Samples

  • Akl, Magda Ali
    • Bulletin of the Korean Chemical Society
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    • v.27 no.5
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    • pp.725-732
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    • 2006
  • A rapid flotation methodology for zinc(II) separation and enrichment from human biofluids is established. At pH 6.0 and ambient temperature, using oleic acid (HOL) as a foaming reagent, zinc(II) was separated with phenanthraquinone monophenyl thiosemicarbazone (PPT) as a new flotation collector for Zn(II). The floated red colored 1 : 2 Zn(II)-PPT complex was measured spectrophotometrically at 526 nm with a molar absorptivity of $1.83 \;{\times}\; 10^5\; L$ mol $L ^{-1}\;cm ^{-1}$. Beer's law was obeyed over a concentration range 0.05-1.0 mg $L ^{-1}$ in the aqueous as well as in the scum layers. The proposed preconcentration flotation methodology was applied to determine Zn(II) in human biofluids. Application was, also, extended to determine Zn(II) in pharmaceutical samples and natural water samples spiked with known amounts of Zn(II) with a preconcentration factor of 100 and a detection limit of 10 ng m$L ^{-1}$. The method was verified by comparison of the spectrophotometric results with flame atomic absorption spectrometric (AAS) measurements. Moreover a postulation for the mechanism of flotation is proposed.

Development and Applications of a Chemical Method for Sequential Analysis of Reducing Oligosaccharides

  • Hong, Seon-Pyo;Lee, Yong-Moon;Hiroshi-Nakamura
    • Archives of Pharmacal Research
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    • v.20 no.2
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    • pp.184-190
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    • 1997
  • A new method based on the chemical reaction has been devised for the sequential analysis of reducing oligosaccharides using 8-amino-2-naphthalenesulfonic acid (ANS), a fluorescent precolumn derivatization reagent for reducing saccharides. The procedure established includes 1) the derivatization of a reducing oligosaccharide to produce a Schiff base, 2) the reduction of the base with sodium cyanoborohydride $(NaBH_3/CN), 3)$ the methoxycarbonylation of the resultant secondary amino group, 4) the cleavage of the glycoside bond next to the reducing end, based on the intramolecular acid hydrolysis by the action of a sulfonic acid group of the ANS derivative, 5) the identification of the liberated reducing end by high-performance liquid chromatography (HPLC), and finally 6) the recovery of the resultant oligosaccharide fragment from the cleavage reaction mixture. The extensive examination of the conditions for the sequential analysis of reducing oligosaccharides resulted in the procedure of simplicity , high selectivity and high recovery. This procedure was found to be useful for the sequential analysis of di-, tri- and tetrasaccharides.

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On-Line Measurement System for the Determination of Chemical Oxygen Demand (화학적 산소 요구량 측정을 위한 On-Line 측정 시스템에 관한 연구)

  • 정형근;차기철
    • Journal of Environmental Science International
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    • v.7 no.2
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    • pp.203-208
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    • 1998
  • A simple on-line measurement system consisting of a conventional peristaltic pump, a HPLC-type heater, and a flow-through spectrophotometer is introduced for the determination of chemical oxygen demand(CODI. The system was configured such that the reaction mixture in the highly concentrated surffuric acrid medium flowing through the PTFE reaction tubing was heated at 150℃ and the absorbance of dichromate was continuously moutored at 445 m. The same addation principle as in the standard procedure was employed akcept the use of CoSO4 as a new effective catalyst. To test the system, potassium hydrogen phthalate was selected as a COD standard material. With suitably optimized reaction condition, the applicable concentration range depends on the concentration of potassium dichromate in the oxidizing reagent. With 2.0×10-3 M and 5.0×10-4M dichromate, the linear dynamic range was observed up to 400 ppm and 100 ppm, respectively. The standards in the Unear ranges were shown to be completely oxidized, which was confirmed with sodium oxalate or Mohr's salt. In all cases, the typical reproduclbility for betweenruns was 2% or less. The proposed measurement system provides the valuable in- formation for the further development of automated analysis system based on the present standard procedure.

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A Study on The Synthesis of Camostat Mesylate Using Vilsmeier-Haack Reaction (Vilsmeier-Haack 반응을 이용한 Camostat Mesylate의 합성법 연구)

  • Kim, Dong Nyeon;Kim, Seok Chan
    • Applied Chemistry for Engineering
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    • v.33 no.4
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    • pp.440-443
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    • 2022
  • A key step in the synthesis of camostat mesylate, which is most widely used as a treatment for chronic pancreatitis, was conducted. Camostat mesylate was synthesized through the esterification reaction of two intermediates, GBA (4-guanidinobenzoic acid hydrochloride) and DOHA [2-(dimethylamino)-2-oxoethyl-2-(4-hydroxyphenyl)acetate]. In order to overcome the problem raised due to the low yield and expensive reagents, a new economical synthesis method was developed that can produce camostat mesylate with a high yield of 80% by activating the acid functional group of GBA using the Vilsmeier-Haack reaction and coupling it with DOHA.

Application of SiO2 nanocomposite ferroelectric material in preparation of trampoline net for physical exercise

  • Zhanguo Su;Junyan Meng;Yiping Su
    • Advances in nano research
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    • v.14 no.4
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    • pp.355-362
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    • 2023
  • Physical exercise, especially intense exercise and high intensity interval training (HIIT) by trampoline, can lead to muscle injuries. These effects can be reduced with intelligent products made of nanocomposite materials. Most of these nanocomposites are polymers reinforced with silicon dioxide, alumina, and titanium dioxide nanoparticles. This study presents a polymer nanocomposite reinforced with silica. As a result of the rapid reaction between tetraethyl orthosilicate and ammonia in the presence of citric acid and other agents, silica nanostructures were synthesized. By substituting bis (4-amino phenoxy) phenyl-triptycene in N, N-dimethylformamide with potassium carbonate, followed by catalytic reduction with hydrazine and Pd/C, the diamine monomer bis (4-amino phenoxy) phenyl-triptycene is prepared. We synthesized a new polyaromatic (imide) with triptycene unit by sol-gel method from aromatic diamines and dianhydride using pyridine as a condensation reagent in NMP. PI readily dissolves in solvents and forms robust and tough polymer films in situ. The FTIR and NMR techniques were used to determine the effects of SiO2 on the sol-gel process and the structure of the synthesized nanocomposites. By using a simultaneous thermal analysis (DTA-TG) method, the appropriate thermal operation temperature was also determined. Through SEM analysis, the structure, shape, size, and specific surface area of pores were determined. Analysis of XRD results is used to determine how SiO2 affects the crystallization of phases and the activation energy of crystallization.

A Study on the Durable Press Finishing of Cotton Fiber Treated with Polycarboxylic Acid (폴리카르복시 산 처리 면섬유의 DP가공에 관한 연구)

  • 이찬민;최철민
    • Textile Coloration and Finishing
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    • v.9 no.6
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    • pp.58-67
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    • 1997
  • PTCA(1,2,3-propanetricarboxylic acid) and BTCA(1,2,3-butanetetracarboxylic acid) are selected as new nonformaldehyde agents for ester crosslinking of cotton cellulose to replace the traditional DMDHEU reagent. A goal of this research is to propose unknown ester mechanism of cotton cellulose by PTCA or BTCA using crystal structure model suggested by Meyer and Takahashi. In pursuit of these goals, we have treated 100% cotton broad cloth with PTCA or BTCA and different catalysts. They were used with $NaH_2PO_2,\;NaH_2PO_4,\;Na_2HPO_4,\;NaH_2PO_2,\;Na_3PO_4,$ catalysts to produce nonformaldehyde fabric finishes. Treatments were applied to all cotton fabrics using a pad-dry -cure process. The esterfication of cotton treated with BTCA or PTCA was investigated using Fourier transform infrared(FT-IR) spectra and the breaking strength, abrasion retention and discoloration properties were determined to prove the durable finished fabrics. Patterns with respect to abrasion resistance were more complex. Because PTCA and BTCA add-ons were comparable, the data suggest that the more effective catalysts, $NaH_2PO_2$ and mixed phosphate $NaH_2PO_2/NaH_2PO_4$) are effecting either a great number of crosslinks in the cotton or producing crosslinks that differ in actual structure.

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